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Process for the preparation of N-(2-((2- (dimethylamino)ethyl)(methyl)amino)-4-methoxy-5-((4-(1-methyl- 1H-indol-3-yl)pyrimidin-2-yl)amino)phenyl)acrylamide ethanesulfonate

IP.com Disclosure Number: IPCOM000249395D
Publication Date: 2017-Feb-23
Document File: 4 page(s) / 94K

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The IP.com Prior Art Database

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Process for the preparation of N-(2-((2- (dimethylamino)ethyl)(methyl)amino)-4-methoxy-5-((4-(1-methyl-

1H-indol-3-yl)pyrimidin-2-yl)amino)phenyl)acrylamide ethanesulfonate

Provided herein is a process for preparing N-(2-((2- (dimethylamino)ethyl)(methyl)amino)-4-methoxy-5-((4-(1-methyl-1H-indol-3- yl)pyrimidin-2-yl)amino)phenyl)acrylamide ethanesulfonate referred herein as compound (1), having the following structure:

N

N

N

N H

NH

N

N

O

O CH3CH2SO3H

(1)  

 

Enclosed herein after is crystalline form of Compound (1). Compound (1) can be isolated in polymorphic form I. The above described process may provide Compound (1) having a purity of 99.9% or higher.

Figure 1: An XRPD pattern of crystalline form I of Compound (1), prepared according to Example 1

 

Main peaks ± 0.2 deg 2-Theta of crystalline form I of Compound (1):

Peak Position [deg 2-Theta]

7.1 8.4 9.0 10.4 14.8 16.1 16.4 17.2 17.6 18.2 18.8 19.1 19.5 19.6 20.2 20.9 21.1 21.4

5 10 15 20 25 30 35 40 2Theta (°)

0

100

200

300

400

500

In te

ns ity

(c ps

)

22.0 22.4 23.0 24.0 24.2 24.7 25.0 25.8 26.3 27.6

 

Experimental part:

XRPD method:

Powder X-ray Diffraction was performed on PANalytical Empyrean X-Ray

powder diffractometer; CuKα radiation (λ = 1.541874 Å); X'Celerator detector;

laboratory temperature 25 ± 2 °C; zero background sample holders. Prior to analysis,

the samples were gently ground using a mortar and pestle to obtain a fine powder. The

ground sample was adjusted into a cavity of the sample holder and the surface of the

sample was smoothed using a cover glass.

Measurement parameters:

Scan range 3 – 40 degrees 2-theta

S...